Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 2-Methyl-2-nitro-1,3-propanediol ditriflate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 2-Methyl-2-nitro-1,3-propanediol | HCID 6480 | — |
| 반응물 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 2-Methyl-2-nitro-1,3-propanediol ditriflate | HCID 59393620 | — |
반응 단계
To a solution of triflic anhydride (16.5 ml, 0.1 mol) in chloroform (50 ml) is added a solution of 2-methyl-2-nitro-1,3-propanediol (6.75 g, 0.05 mol) and pyridine (8.85 ml, 0.11 mol) in chloroform (50 ml) with external cooling to ensure a temperature of between 0° and 5° C. during the addition. After the addition the cooling bath is removed and the reaction stirred for 18 hours at ambient temperature. The reaction mixture is transferred to a separating funnel and washed with water. The organic layer is dried (Na2SO4), filtered and evaporated to dryness. The crude product is purified by chromatography using a 4:1 mixture of Hexane:Ethyl acetate as eluant; the product is obtained as a solid with melting point 50-52° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08084474B2 |
| 출처 데이터셋 | uspto-grants-2011_12 |
| ORD ID | ord-ada0034dde9c449e94832228aecc81c6 |
| 출처 메모 | uspto-grants-2011_12 |